#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/72/2207222.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2207222
loop_
_publ_author_name
'Zhu, Long-Guan'
'Xiao, Hong-Ping'
_publ_section_title
;
 Poly[aqua(2,2'-bipyridine)(μ₃-3-sulfonatobenzoato)lead(II)]
;
_journal_coeditor_code           FL6194
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2283
_journal_page_last               m2285
_journal_paper_doi               10.1107/S1600536805032289
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Pb (C7 H4 O5 S) (C10 H8 N2) (H2 O)]'
_chemical_formula_moiety         'C17 H14 N2 O6 Pb S'
_chemical_formula_sum            'C17 H14 N2 O6 Pb S'
_chemical_formula_weight         581.55
_chemical_name_systematic
;
Poly[aqua(2,2'-bipyridine)(μ₃-3-sulfonatobenzoato)lead(II)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                98.2270(10)
_cell_angle_beta                 98.1470(10)
_cell_angle_gamma                102.2320(10)
_cell_formula_units_Z            2
_cell_length_a                   7.0098(4)
_cell_length_b                   11.2360(7)
_cell_length_c                   11.6818(7)
_cell_measurement_reflns_used    3723
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.8
_cell_volume                     875.75(9)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.038
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4803
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         1.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.791
_exptl_absorpt_correction_T_max  0.508
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    2.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.083
_refine_diff_density_min         -1.550
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3210
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.034
_refine_ls_R_factor_gt           0.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0524P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.077
_refine_ls_wR_factor_ref         0.078
_reflns_number_gt                3069
_reflns_number_total             3210
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fl6194.cif
_cod_data_source_block           I
_cod_database_code               2207222
_cod_database_fobs_code          2207222
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Pb1 0.85100(3) 0.297872(17) 0.343132(17) 0.02389(10) Uani d . 1 Pb
S1 1.2550(2) 0.40708(13) 0.63256(14) 0.0276(3) Uani d . 1 S
O1 0.8992(7) -0.1562(4) 0.6653(5) 0.0439(12) Uani d . 1 O
O2 1.2099(7) -0.0650(4) 0.6664(4) 0.0381(11) Uani d . 1 O
O3 1.2025(8) 0.4411(4) 0.5183(4) 0.0432(12) Uani d . 1 O
O4 1.4422(7) 0.3725(4) 0.6468(5) 0.0492(14) Uani d . 1 O
O5 1.2413(7) 0.5009(4) 0.7282(4) 0.0362(11) Uani d . 1 O
O6 0.4922(8) 0.2836(5) 0.4024(5) 0.0525(13) Uani d D 1 O
N1 0.6353(7) 0.2116(4) 0.1454(4) 0.0321(12) Uani d . 1 N
N2 1.0125(8) 0.3380(5) 0.1689(4) 0.0317(11) Uani d . 1 N
C1 1.0310(9) -0.0629(5) 0.6591(5) 0.0280(13) Uani d . 1 C
C2 0.9741(9) 0.0571(5) 0.6474(5) 0.0275(13) Uani d . 1 C
C3 1.1206(9) 0.1610(5) 0.6457(5) 0.0256(12) Uani d . 1 C
H3 1.2520 0.1557 0.6499 0.031 Uiso calc R 1 H
C4 1.0698(9) 0.2736(5) 0.6375(5) 0.0239(12) Uani d . 1 C
C5 0.8745(9) 0.2820(6) 0.6322(6) 0.0305(13) Uani d . 1 C
H5 0.8423 0.3580 0.6302 0.037 Uiso calc R 1 H
C6 0.7263(9) 0.1770(6) 0.6300(6) 0.0333(14) Uani d . 1 C
H6 0.5946 0.1820 0.6230 0.040 Uiso calc R 1 H
C7 0.7754(10) 0.0648(6) 0.6381(6) 0.0333(14) Uani d . 1 C
H7 0.6766 -0.0053 0.6373 0.040 Uiso calc R 1 H
C8 0.4499(11) 0.1463(7) 0.1399(7) 0.0473(18) Uani d . 1 C
H8 0.4085 0.1298 0.2094 0.057 Uiso calc R 1 H
C9 0.3166(13) 0.1020(9) 0.0349(8) 0.065(2) Uani d . 1 C
H9 0.1879 0.0572 0.0328 0.078 Uiso calc R 1 H
C10 0.3832(15) 0.1272(10) -0.0640(8) 0.074(3) Uani d . 1 C
H10 0.2984 0.0981 -0.1360 0.089 Uiso calc R 1 H
C11 0.5743(12) 0.1952(8) -0.0615(6) 0.055(2) Uani d . 1 C
H11 0.6167 0.2138 -0.1301 0.066 Uiso calc R 1 H
C12 0.7000(10) 0.2346(6) 0.0465(5) 0.0349(14) Uani d . 1 C
C13 0.9078(10) 0.3041(6) 0.0590(6) 0.0347(14) Uani d . 1 C
C14 0.9941(12) 0.3334(8) -0.0361(7) 0.055(2) Uani d . 1 C
H14 0.9213 0.3092 -0.1120 0.066 Uiso calc R 1 H
C15 1.1890(14) 0.3988(9) -0.0169(8) 0.068(3) Uani d . 1 C
H15 1.2480 0.4194 -0.0801 0.081 Uiso calc R 1 H
C16 1.2955(12) 0.4332(8) 0.0942(7) 0.058(2) Uani d . 1 C
H16 1.4275 0.4769 0.1083 0.070 Uiso calc R 1 H
C17 1.2016(10) 0.4014(6) 0.1856(7) 0.0405(15) Uani d . 1 C
H17 1.2729 0.4251 0.2619 0.049 Uiso calc R 1 H
H6A 0.500(9) 0.333(5) 0.466(4) 0.050 Uiso d D 1 H
H6B 0.374(4) 0.240(6) 0.381(6) 0.050 Uiso d D 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Pb1 O1 2_756 2_756 50.53(14) yes
O1 Pb1 O3 2_756 . 76.52(15) yes
O1 Pb1 O5 2_756 2_766 143.95(15) yes
O1 Pb1 O6 2_756 . 136.36(17) yes
N1 Pb1 O1 . 2_756 98.92(16) yes
N2 Pb1 O1 . 2_756 74.58(16) yes
O2 Pb1 O3 2_756 . 113.63(14) yes
O2 Pb1 O5 2_756 2_766 151.96(15) yes
O2 Pb1 O6 2_756 . 87.76(16) yes
N1 Pb1 O2 . 2_756 76.70(15) yes
N2 Pb1 O2 . 2_756 104.73(16) yes
O5 Pb1 O3 2_766 . 94.41(14) yes
O6 Pb1 O3 . . 117.93(15) yes
N1 Pb1 O3 . . 158.46(15) yes
N2 Pb1 O3 . . 94.25(15) yes
O6 Pb1 O5 . 2_766 78.85(17) yes
N1 Pb1 O5 . 2_766 76.79(15) yes
N2 Pb1 O5 . 2_766 71.37(15) yes
N1 Pb1 O6 . . 80.07(16) yes
N2 Pb1 O6 . . 137.58(18) yes
N1 Pb1 N2 . . 64.39(16) yes
O4 S1 O5 . . 113.1(3) ?
O4 S1 O3 . . 112.9(3) ?
O5 S1 O3 . . 111.7(3) ?
O4 S1 C4 . . 106.9(3) ?
O5 S1 C4 . . 105.6(3) ?
O3 S1 C4 . . 106.0(3) ?
C1 O1 Pb1 . 2_756 91.6(4) ?
C1 O2 Pb1 . 2_756 94.8(3) ?
S1 O3 Pb1 . . 122.6(2) ?
S1 O5 Pb1 . 2_766 113.6(2) ?
Pb1 O6 H6A . . 111(4) ?
Pb1 O6 H6B . . 140(4) ?
H6A O6 H6B . . 109(6) ?
C8 N1 C12 . . 119.8(6) ?
C8 N1 Pb1 . . 119.1(5) ?
C12 N1 Pb1 . . 121.1(4) ?
C17 N2 C13 . . 119.1(6) ?
C17 N2 Pb1 . . 119.8(4) ?
C13 N2 Pb1 . . 121.0(4) ?
O2 C1 O1 . . 122.3(5) ?
O2 C1 C2 . . 118.3(5) ?
O1 C1 C2 . . 119.3(6) ?
C3 C2 C7 . . 119.9(5) ?
C3 C2 C1 . . 119.2(5) ?
C7 C2 C1 . . 120.8(5) ?
C2 C3 C4 . . 119.7(5) ?
C2 C3 H3 . . 120.2 ?
C4 C3 H3 . . 120.2 ?
C5 C4 C3 . . 120.3(5) ?
C5 C4 S1 . . 119.4(4) ?
C3 C4 S1 . . 120.2(5) ?
C4 C5 C6 . . 120.1(5) ?
C4 C5 H5 . . 120.0 ?
C6 C5 H5 . . 120.0 ?
C7 C6 C5 . . 119.9(6) ?
C7 C6 H6 . . 120.0 ?
C5 C6 H6 . . 120.0 ?
C6 C7 C2 . . 120.0(6) ?
C6 C7 H7 . . 120.0 ?
C2 C7 H7 . . 120.0 ?
N1 C8 C9 . . 122.9(7) ?
N1 C8 H8 . . 118.6 ?
C9 C8 H8 . . 118.6 ?
C10 C9 C8 . . 116.6(8) ?
C10 C9 H9 . . 121.7 ?
C8 C9 H9 . . 121.7 ?
C9 C10 C11 . . 122.0(8) ?
C9 C10 H10 . . 119.0 ?
C11 C10 H10 . . 119.0 ?
C12 C11 C10 . . 118.0(7) ?
C12 C11 H11 . . 121.0 ?
C10 C11 H11 . . 121.0 ?
N1 C12 C11 . . 120.6(7) ?
N1 C12 C13 . . 116.8(6) ?
C11 C12 C13 . . 122.6(6) ?
N2 C13 C14 . . 120.7(7) ?
N2 C13 C12 . . 116.4(6) ?
C14 C13 C12 . . 122.9(6) ?
C15 C14 C13 . . 119.3(7) ?
C15 C14 H14 . . 120.4 ?
C13 C14 H14 . . 120.4 ?
C16 C15 C14 . . 120.2(7) ?
C16 C15 H15 . . 119.9 ?
C14 C15 H15 . . 119.9 ?
C15 C16 C17 . . 118.0(8) ?
C15 C16 H16 . . 121.0 ?
C17 C16 H16 . . 121.0 ?
N2 C17 C16 . . 122.8(7) ?
N2 C17 H17 . . 118.6 ?
C16 C17 H17 . . 118.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 O1 2_756 2.607(4) yes
Pb1 O2 2_756 2.543(4) yes
Pb1 O3 . 2.966(5) yes
Pb1 O5 2_766 2.689(4) yes
Pb1 O6 . 2.680(5) yes
Pb1 N1 . 2.511(5) yes
Pb1 N2 . 2.515(5) yes
S1 O3 . 1.459(5) yes
S1 O4 . 1.440(5) yes
S1 O5 . 1.451(5) yes
S1 C4 . 1.777(6) no
O1 C1 . 1.260(7) yes
O1 Pb1 2_756 2.607(4) no
O2 C1 . 1.250(8) yes
O2 Pb1 2_756 2.543(4) ?
O5 Pb1 2_766 2.689(4) ?
O6 H6A . 0.85(5) ?
O6 H6B . 0.85(5) ?
N1 C8 . 1.338(9) ?
N1 C12 . 1.339(8) ?
N2 C17 . 1.338(9) ?
N2 C13 . 1.344(8) ?
C1 C2 . 1.504(8) ?
C2 C3 . 1.387(8) ?
C2 C7 . 1.404(9) ?
C3 C4 . 1.398(8) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.385(8) ?
C5 C6 . 1.391(9) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.387(8) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
C8 C9 . 1.389(11) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.350(13) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.389(13) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.386(9) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.476(10) ?
C13 C14 . 1.385(9) ?
C14 C15 . 1.377(12) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.361(12) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.381(10) ?
C16 H16 . 0.9300 ?
C17 H17 . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O6 H6A O4 1_455 0.85(5) 2.21(4) 2.982(8) 151(6) yes
O6 H6B O1 2_656 0.85(5) 1.91(5) 2.756(7) 175(7) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O4 S1 O3 Pb1 . . 115.9(3)
O5 S1 O3 Pb1 . . -115.3(3)
C4 S1 O3 Pb1 . . -0.8(4)
N1 Pb1 O3 S1 . . -153.6(3)
N2 Pb1 O3 S1 . . -146.6(3)
O2 Pb1 O3 S1 2_756 . -38.5(4)
O1 Pb1 O3 S1 2_756 . -73.6(3)
O6 Pb1 O3 S1 . . 62.1(4)
O5 Pb1 O3 S1 2_766 . 141.8(3)
O4 S1 O5 Pb1 . 2_766 125.0(3)
O3 S1 O5 Pb1 . 2_766 -3.7(4)
C4 S1 O5 Pb1 . 2_766 -118.5(3)
N2 Pb1 N1 C8 . . 178.1(6)
O2 Pb1 N1 C8 2_756 . 64.3(5)
O1 Pb1 N1 C8 2_756 . 110.0(5)
O6 Pb1 N1 C8 . . -25.7(5)
O5 Pb1 N1 C8 2_766 . -106.5(5)
O3 Pb1 N1 C8 . . -174.2(4)
N2 Pb1 N1 C12 . . -4.9(4)
O2 Pb1 N1 C12 2_756 . -118.7(5)
O1 Pb1 N1 C12 2_756 . -72.9(5)
O6 Pb1 N1 C12 . . 151.3(5)
O5 Pb1 N1 C12 2_766 . 70.6(5)
O3 Pb1 N1 C12 . . 2.9(7)
N1 Pb1 N2 C17 . . -179.9(5)
O2 Pb1 N2 C17 2_756 . -112.8(5)
O1 Pb1 N2 C17 2_756 . -71.8(5)
O6 Pb1 N2 C17 . . 144.1(4)
O5 Pb1 N2 C17 2_766 . 96.2(5)
O3 Pb1 N2 C17 . . 3.0(5)
N1 Pb1 N2 C13 . . 4.8(4)
O2 Pb1 N2 C13 2_756 . 71.9(5)
O1 Pb1 N2 C13 2_756 . 112.9(5)
O6 Pb1 N2 C13 . . -31.3(6)
O5 Pb1 N2 C13 2_766 . -79.1(5)
O3 Pb1 N2 C13 . . -172.3(5)
Pb1 O2 C1 O1 2_756 . 9.0(7)
Pb1 O2 C1 C2 2_756 . -173.5(5)
Pb1 O1 C1 O2 2_756 . -8.8(6)
Pb1 O1 C1 C2 2_756 . 173.8(5)
O2 C1 C2 C3 . . -0.3(9)
O1 C1 C2 C3 . . 177.3(6)
O2 C1 C2 C7 . . 179.6(6)
O1 C1 C2 C7 . . -2.8(9)
C7 C2 C3 C4 . . 1.5(9)
C1 C2 C3 C4 . . -178.6(5)
C2 C3 C4 C5 . . 0.6(9)
C2 C3 C4 S1 . . -178.9(4)
O4 S1 C4 C5 . . 176.5(5)
O5 S1 C4 C5 . . 55.8(5)
O3 S1 C4 C5 . . -62.8(5)
O4 S1 C4 C3 . . -3.9(6)
O5 S1 C4 C3 . . -124.6(5)
O3 S1 C4 C3 . . 116.7(5)
C3 C4 C5 C6 . . -2.8(9)
S1 C4 C5 C6 . . 176.7(5)
C4 C5 C6 C7 . . 2.8(10)
C5 C6 C7 C2 . . -0.6(10)
C3 C2 C7 C6 . . -1.5(9)
C1 C2 C7 C6 . . 178.6(6)
C12 N1 C8 C9 . . -1.3(11)
Pb1 N1 C8 C9 . . 175.8(7)
N1 C8 C9 C10 . . 0.5(14)
C8 C9 C10 C11 . . -0.8(16)
C9 C10 C11 C12 . . 1.9(16)
C8 N1 C12 C11 . . 2.4(10)
Pb1 N1 C12 C11 . . -174.6(5)
C8 N1 C12 C13 . . -178.3(6)
Pb1 N1 C12 C13 . . 4.7(7)
C10 C11 C12 N1 . . -2.6(12)
C10 C11 C12 C13 . . 178.1(8)
C17 N2 C13 C14 . . 0.5(10)
Pb1 N2 C13 C14 . . 175.8(6)
C17 N2 C13 C12 . . -179.9(6)
Pb1 N2 C13 C12 . . -4.5(7)
N1 C12 C13 N2 . . -0.1(9)
C11 C12 C13 N2 . . 179.2(7)
N1 C12 C13 C14 . . 179.5(7)
C11 C12 C13 C14 . . -1.2(11)
N2 C13 C14 C15 . . -0.5(12)
C12 C13 C14 C15 . . 179.9(8)
C13 C14 C15 C16 . . 0.5(15)
C14 C15 C16 C17 . . -0.5(15)
C13 N2 C17 C16 . . -0.5(10)
Pb1 N2 C17 C16 . . -175.9(6)
C15 C16 C17 N2 . . 0.5(13)
